反应详情

A mixture of 4-chloro-2-iodoaniline (0.5 g, 1.97 mmol), 1,3-cyclohexanedione (0.22 g, 1.96 mmol) and p-toluenesulfonic acid monohydrate (catalytic) in toluene (6 mL) were heated to reflux for 2 h. The reaction was cooled and EtOAc (50 mL) was added and the organic phase was washed with water (20 mL) and brine (20 mL), dried over sodium sulfate, filtered and evaporated to give a brown solid, which was purified by column chromatography [Silica, eluent: EtOAc:hexane to give 3-(4-chloro-2-iodophenylamino)cyclohex-2-enone as a yellow solid (0.55 g, 80%).

1. temperaturewere heated
2. temperatureto reflux for 2 h
3. temperatureThe reaction was cooled
4. washthe organic phase was washed with water (20 mL) and brine (20 mL)
5. dry with materialdried over sodium sulfate
6. filtrationfiltered
7. customevaporated
8. customto give a brown solid, which
9. customwas purified by column chromatography [Silica, eluent